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Synthesizing method of vinylsilane

A technology of vinyl silane and vinyl trichlorosilane, which is applied in the field of synthesis of vinyl silane, can solve the problems affecting the heat resistance and dielectric properties of cross-linked polyethylene materials, and the decline in electrical properties, so as to improve heat resistance and Effects of dielectric properties, small steric hindrance, and high hydrolysis rate

Inactive Publication Date: 2019-02-12
江西晨光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] As a general-purpose silane coupling agent, vinyl trialkoxysilane is widely used in silane cross-linked polyethylene materials such as cables and wires, heat-resistant pipes, heat-resistant hoses and films, to improve the electrical and mechanical properties of cross-linked polymers , but under high humidity conditions, the electrical properties will decrease due to water absorption, and the amount of vinyl silane added can reach up to 2.5%. performance

Method used

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  • Synthesizing method of vinylsilane

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preparation example Construction

[0016] A method for synthesizing vinyl silane, the specific steps of which are: adding lower alcohols into a container at room temperature, slowly adding vinyl trichlorosilane and silicon tetrachloride dropwise under stirring, cooling with ethanol cooling liquid, and condensing The upper port of the pipe is connected to the tail gas absorption device. After the dropwise addition, the temperature is raised to reflux the lower alcohol for a period of time, the temperature is lowered to test and the pH of the reaction solution is adjusted, and a certain concentration of alcohol aqueous solution is slowly added dropwise. Lower the temperature and neutralize to a pH value of 6-7, filter, distill the filtrate under reduced pressure to recover uncondensed tetraalkoxysilane and vinyl alkoxysilane, and rectify to obtain the vinyl silane product.

[0017] The molar ratio of vinyltrichlorosilane to silicon tetrachloride is 1:1.

[0018] The molar ratio of the molar sum of the vinyltrichl...

Embodiment 1

[0029] Embodiment 1: (methanol: silicon chloride=17.85:1, alcohol water concentration 30%)

[0030] Vinylsilane synthesis: add 2kg of industrial methanol to a 5L four-necked flask, add 565.25g of vinyltrichlorosilane (3.5mol) and 564.65g of silicon tetrachloride dropwise through a constant pressure dropping funnel under stirring, Control the esterification temperature ≤ 20°C, condense the ethanol cooling liquid at -15-0°C, connect the condensation pipe to the tail gas absorption device, slowly raise the temperature until the methanol is refluxed for 2 hours, cool down to 40°C and test the pH to 2, add 3ml of 28% methanol Adjust the pH to 3-4 with aqueous sodium methanol solution, add dropwise a mixture of 63g water and 147g methanol, hydrolyze at a temperature of 38-40°C, add dropwise for 2.5 hours, heat up and reflux for 3 hours after hydrolysis, recover methanol by distillation, and distill at 110°C The amount of methanol produced was significantly reduced. Change the receiv...

Embodiment 2

[0032] Embodiment 2: (methanol; silicon chloride=22.92; 1, alcohol water concentration 50%)

[0033] Synthesis of vinyl silane: Add 2.2 kg of acidic methanol with a pH of 6 to recover from esterification into a 5L four-necked flask, and add 484.5 g of vinyl trichlorosilane (3 mol) and 509.7 g of tetrachlorosilane simultaneously through a constant pressure dropping funnel under stirring. Silicon chloride, ice-salt bath to control esterification temperature ≤ 20°C, -15-0°C ethanol cooling liquid to condense, condensing pipe port to tail gas absorption device, after adding, slowly raise the temperature to make the methanol reflux for 4 hours, cool down to 40°C and test the pH as 3. Add 0.4ml triethylamine to adjust the pH to 3-4, add dropwise a mixture of 54g water and 55g recovered acidic methanol, hydrolyze the temperature at about 42°C, add dropwise for 3h, heat up and reflux for 3h after hydrolysis, distill and recover methanol, When the temperature reaches 110°C, the distill...

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Abstract

The invention discloses a synthesizing method of vinylsilane. The synthesizing method specifically comprises the following steps of adding low-grade alcohol into a container at room temperature, stirring, respectively dropwise adding trichlorovinylsilane and silicon tetrachloride, cooling by ethanol cooling liquid, and connecting a tail gas absorbing device to an upper opening of a condensing pipe; after dropwise adding is finished, warming, refluxing the low-grade alcohol for a period of time, cooling, testing and adjusting the pH (potential of hydrogen) value of the reaction liquid, and slowly dropwise adding an alcohol-water solution with a certain concentration; after adding is finished, refluxing, performing condensation reaction while collecting the alcohol, cooling, neutralizing thepH value to 6 to 7, and filtering; performing reduced pressure distillation on the filtrate, centrally recycling the uncondensed tetraalkoxysilane and vinyl alkoxysilane, rectifying, and collecting,so as to obtain a vinylsilane product. The synthesizing method has the advantages that the steps are simple, and the yield rate is high; the yield rate can reach 96% after direct esterification, hydrolysis, condensation, distillation and purification; the byproduct can be directly recycled, the pollution to environment is avoided, and the energy-saving and environment-friendly effects are realized.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing vinyl silane. Background technique [0002] As a general-purpose silane coupling agent, vinyl trialkoxysilane is widely used in silane cross-linked polyethylene materials such as cables and wires, heat-resistant pipes, heat-resistant hoses and films, to improve the electrical and mechanical properties of cross-linked polymers , but under high humidity conditions, the electrical properties will decrease due to water absorption, and the amount of vinyl silane added can reach up to 2.5%. performance. Tetraalkoxysilane can be used in the synthesis of MQ silicone resin, high-temperature resistant coatings, as a crosslinking agent for electronic silicone rubber, and as a dry moisture-proof treatment agent for dewatering inorganic zinc-rich coatings, adhesives, etc. [0003] Reaction of vinyltrichlorosilane and silicon tetrachloride with alcohol / water simulta...

Claims

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Application Information

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IPC IPC(8): C07F7/18C08L23/08C08K5/14C08K5/5425C08J3/24
CPCC07F7/188C08J3/24C08J2323/08C08K5/14C08K5/5425
Inventor 丁冰杨静梁秋鸿周煜华周俊
Owner 江西晨光新材料股份有限公司
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